A validated liquid chromatography/tandem mass spectrometry method for the analysis of efavirenz in 0.2 mg hair samples from human immunodeficiency virus infected patients

Johnston Jenna; Orrell Catherine; Smith Peter; Joubert Anton; Wiesner Lubbe

摘要

Rationale >Drug levels in hair provide a longer window of detection, compared to plasma drug levels, and therefore hair analysis has the advantage of assessing adherence over a longer period of time. No methods for the analysis of antiretroviral drugs in hair currently exist in South Africa, and worldwide there is only one validated method for the determination of efavirenz in hair that has been published. </section> <section xml:id="rcm8077-sec-0002" numbered="no"> <title type="main">Methods >Efavirenz was extracted from 0.2?mg of hair through a simultaneous pulverization and extraction step. Separation was achieved on an Agilent Poroshell C18 column using an isocratic elution with a total run time of 3?min. A triple quadrupole mass spectrometer set to electrospray ionization in positive multiple reaction monitoring mode was used for detection. The method was validated over the concentration range 0.625–40?ng/mg. </section> <section xml:id="rcm8077-sec-0003" numbered="no"> <title type="main">Results >Using ten times less hair than in a previously published method, the lower limit of quantitation was validated at 0.625?ng/mg. The interday and intraday assay precision, expressed as the percentage coefficient of variation (CV), for spiked calibration standards and quality control samples was lower than 7% and accuracy ranged from 97 to 110%. For quality controls prepared from authentic hair the CV was less than 12%. The extraction efficiency for authentic quality control samples was determined to be 83% after repeated extractions of the same samples. </section> <section xml:id="rcm8077-sec-0004" numbered="no"> <title type="main">Conclusions >This p </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> <div class="translation abstracttxt"> <span class="zhankaihshouqi fivelineshidden" id="abstract"> <span>机译：</span><abstract xmlns =“http://www.wiley.com/namespaces/wiley”type =“main”xml：lang =“en”> <section xml：id =“rcm8077-sec-0001”编号=“否” > <标题类型=“main”>理性</标题> >头发的药物水平提供更长的检测窗口，与血浆药物水平相比，毛发分析具有在更长的时间内评估粘附的优点。没有关于南非目前存在于头发的抗逆转录病毒药物的方法，全球只存在一项验证的方法，用于测定已发表的头发中的eFaviraz。</ p> </ section> <section XML：ID = “RCM8077-SEC-0002”编号=“否”> <标题类型=“main”>方法通过同时粉碎和提取步骤从0.2Ω·mg头发中提取0.2Ω·mg头发。在Agilent Poroshell C18柱上使用等离子洗脱来实现分离，其总运行时间为3？min。用于阳性多反应监测模式下的电喷雾电离的三重四极孔质谱仪进行检测。该方法在浓度范围内验证0.625-40≤ng/ mg。</ p> </ section> <section xml：id =“rcm8077-sec-0003”编号=“否”> <标题类型=“main” >结果</标题> >使用较少的毛发少于先前发表的方法，在0.625μg/ mg时验证了数量下限。表达作为尖刺校准标准和质量控制样品的间隔和盘中测定精度表达为百分比变异系数（CV），低于7％，精度范围为97至110％。对于由正宗的毛发制备的质量控制，CV小于12％。在相同样品的重复萃取后，确定正品质量控制样品的提取效率为83％。</ p> </ section> <secto xml：id =“rcm8077-sec-0004”编号=“否”> <标题类型=“main”>结论</ title> >这个p </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> </div> <div class="record"> <h2 class="all_title" id="enpatent33" >著录项</h2> <ul> <li> <span class="lefttit">来源</span> <div style="width: 86%;vertical-align: text-top;display: inline-block;"> <a href='/journal-foreign-26627/'>《Rapid Communications in Mass Spectrometry: RCM》</a> <b style="margin: 0 2px;">|</b><span>2018年第8期</span><b style="margin: 0 2px;">|</b><span>共8页</span> </div> </li> <li> <div class="author"> <span class="lefttit">作者</span> <p id="fAuthorthree" class="threelineshidden zhankaihshouqi"> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Johnston Jenna&option=202" target="_blank" rel="nofollow">Johnston Jenna;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Orrell Catherine&option=202" target="_blank" rel="nofollow">Orrell Catherine;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Smith Peter&option=202" target="_blank" rel="nofollow">Smith Peter;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Joubert Anton&option=202" target="_blank" rel="nofollow">Joubert Anton;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Wiesner Lubbe&option=202" target="_blank" rel="nofollow">Wiesner Lubbe;</a> </p> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zkzz" style="display: none;">展开▼</span> </div> </li> <li> <div style="display: flex;"> <span class="lefttit">作者单位</span> <div style="position: relative;margin-left: 3px;max-width: 639px;"> <div class="threelineshidden zhankaihshouqi" id="fOrgthree"> <p>Division of Clinical PharmacologyUniversity of Cape TownCape Town South Africa;</p> <p>Desmond Tutu HIV Centre Institute of Infectious Disease and Molecular Medicine and Department of MedicineUniversity of Cape TownCape Town South Africa;</p> <p>Division of Clinical PharmacologyUniversity of Cape TownCape Town South Africa;</p> <p>Division of Clinical PharmacologyUniversity of Cape TownCape Town South Africa;</p> <p>Division of Clinical PharmacologyUniversity of Cape TownCape Town South Africa;</p> </div> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zhdw" style="display: none;">展开▼</span> </div> </div> </li> <li > <span class="lefttit">收录信息</span> <span style="width: 86%;vertical-align: text-top;display: inline-block;"></span> </li> <li> <span class="lefttit">原文格式</span> <span>PDF</span> </li> <li> <span class="lefttit">正文语种</span> <span>eng</span> </li> <li> <span class="lefttit">中图分类</span> <span><a href="https://www.zhangqiaokeyan.com/clc/1187.html" title="分析化学">分析化学;</a></span> </li> <li class="antistop"> <span class="lefttit">关键词</span> <p style="width: 86%;vertical-align: text-top;"> </p> </li> </ul> 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